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投稿时间：2023-09-22
投稿时间：2023-09-22
中文摘要: 采用超高效液相色谱-串联质谱技术，以鸡蛋为研究对象，建立一种高效测定鸡蛋中氟虫腈及其代谢物残留测定方法。样品用乙腈提取，并通过固相萃取技术对样品进行净化处理，供超高效液相色谱-串联质谱仪进行检测。实验结果表明，该方法能够有效地分离和测定氟虫腈及其代谢物残留。在3 个不同的添加水平（0.005、0.010、0.020 mg/kg）下，4 种农药的回收率范围为81.3%～92.5%，相对标准偏差均低于5.5%。；在0.001～0.050 μg/mL 浓度范围内，线性关系良好，相关系数均大于0.990 4；氟虫腈、氟甲腈、氟虫腈砜与氟虫腈亚砜的检出限分别为0.001、0.002、0.002、0.002 mg/kg。该方法准确、灵敏、快速，可满足对鸡蛋中氟虫腈、氟甲腈、氟虫腈砜与氟虫腈亚砜4 种药物残留的检测需要。
Abstract:An efficient and precise method utilizing ultra-high performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS）was developed to quantify fipronil and its metabolites in eggs. The extraction of samples was performed using acetonitrile，followed by solid phase extraction column cleanup to prepare them for UPLC-MS/MS analysis.The results showed good separation，and that the average recovery of fipronil and its metabolites at 0.005，0.010 mg/kg and 0.020 mg/kg was between 81.3% and 92.5%，and the relative standard deviations were below 5.5%. Significant linear correlations were found between the peak area and the concentration of fipronil and its metabolites within the range of 0.001-0.050 μg/mL，with correlation coefficients surpassing 0.990.4. The limit of detection of fipronil，fipronil-desulfinyl，fipronil-sulfide，and fipronilsulfone was 0.001，0.002，0.002 mg/kg and 0.002 mg/kg，respectively.The UPLC-MS/MS method was accurate，sensitive and rapid and can detect fipronil and its metabolites in eggs.
keywords: fipronil fipronil-desulfinyl fipronil-sulfide fipronil-sulfone ultra-high performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS） eggs
文章编号：202404021 中图分类号： 文献标志码：
基金项目:农业农村部财政专项农产品质量安全监管风险评估项目（GJFP2019012、GJFP2019013、GJFP2019019）；2023年海南省自然科学基金项目（323MS092）
| 作者 | 单位 |
| 郭宏斌1，彭侃霖1，吴金玲1，杨舒娴2，林玲1，叶剑芝1，刘元靖1*，王晓芳1 | 1.中国热带农业科学院农产品加工研究所，农业农村部农产品加工质量安全风险评估实验室（湛江），广东湛江 524001；2.云南农业大学热带作物学院，云南普洱 665000 |
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